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Protection Against the Oxidation of Composite Material Parts Containing Carbon and Parts thus Protected

Inactive Publication Date: 2007-08-30
MESSIER BUGATTI INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0007] An object of the invention is to provide a method enabling parts made of composite material containing carbon to be protected against oxidation, the method being easy to implement and being effective even in the presence of oxidation catalysts, in the presence of moisture, and when exposed to high temperatures, greater than 1000° C.
[0009] In known manner, titanium diboride TiB2 behaves as a reservoir for very progressive formation of oxides such as TiO2, B2O3 which are capable of conferring to the protection against oxidation a barrier characteristic against diffusion of oxygen from the surrounding medium, thereby enabling high temperatures to be withstood, i.e. temperatures above 1000° C., and typically up to 1400° C. or higher.
[0010] Above all, by associating with the element phosphorus P present in the composition and with a metal Me coming either from the phosphate precursor used or from exposure to a catalyst for oxidizing carbon and coming from the outside, TiB2 is capable of forming complex oxides of the Ti—O—P-Me type. Forming such oxides thus enables the oxidation catalyst coming from the outside to be trapped in the form of a glass, i.e. above 1000° C. The glass formed in this way also contributes to the oxygen diffusion barrier effect up to at least 1400° C. while being insoluble in water, i.e. while enabling stable protection to be obtained in a moist medium.
[0020] A preliminary step may be performed of treating the composite material part by impregnating it with an aqueous solution of a wetting agent, and then drying the aqueous solution so as to confer on the composite material wettability that is increased by the presence of the wetting agent.
[0021] According to another implementation feature of the method, it may include a step of applying a solution of at least one metal phosphate without any solid filler, prior to applying the composition containing at least a metal phosphate in solution together with titanium diboride, and possibly other solid fillers. Because of its smaller viscosity, the solution that does not have any solid filler, and in particular does not have any titanium diboride, can penetrate more deeply into the residual open internal pores of the composite material. As a result, the protection against oxidation comprises one or more metal phosphates anchored in depth in the pores of the composite material and an association of metal phosphate(s), titanium diboride, and possibly other solid fillers closer to the surface of the composite material.

Problems solved by technology

Whatever the way in which such materials are prepared, they inevitably present residual internal pores that are open and that give oxygen in the surrounding medium access to the core of the material.
The effectiveness of such composition is nevertheless limited above a certain temperature threshold, at around 1000° C., at which temperature the active components of the composition decompose.
Nevertheless, the process of forming complete protection against oxidation then becomes much more complex, since the protection is constituted by two superposed layers, each requiring its own specific implementation process.

Method used

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  • Protection Against the Oxidation of Composite Material Parts Containing Carbon and Parts thus Protected
  • Protection Against the Oxidation of Composite Material Parts Containing Carbon and Parts thus Protected
  • Protection Against the Oxidation of Composite Material Parts Containing Carbon and Parts thus Protected

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0054] Samples of C / C composite material were made as follows.

[0055] Unidirectional fiber sheets of carbon precursor fibers (preoxidized polyacrylonitrile) were superposed in different directions and bonded together by needling as the superposition was being built up. The resulting fiber preform was subjected to heat treatment to transform the precursor into carbon by pyrolysis, and was then densified with a pyrolytic carbon matrix by chemical vapor infiltration. Such a method is well known. Reference can be made, for example, to document U.S. Pat. No. 4,790,052. Samples in the form of rectangular blocks having dimensions of 20 mm×25 mm×8 mm were cut out from the block of C / C material obtained in this way.

[0056] Several samples were provided with protection against oxidation by a process comprising the following steps:

[0057] a) preliminary treatment of the samples by immersing them in an ultrasound vessel containing an aqueous solution of a wetting agent based on polyethoxyl ison...

example 2

[0081] The procedure was as in Example 1, but in step c), an impregnation composition was used containing, in percentage by weight, 32% of Al (H2PO4)3 and 56% ZrB2, the remainder being water.

[0082] Several samples protected using the method of Example 2 were subjected to an oxidation test identical to test V) above.

[0083] Table II below shows the relative mass losses measured on the various samples after performing the observation test (as a percentage relative to initial mass). By way of comparison, Table II shows the mass losses observed in the same oxidation test on samples protected in accordance with Example 1 and on reference protected samples.

TABLE II(Test 1 × 5 h − 650° C. + 1 × 20 min − 1200° +2 × 5 h − 650°)SamplesMass lossProtected in accordance with2.6%Example 12.6%3.4%Protected in accordance with10.1% Example 211.4% 12.5% Reference9.2% 13% 13%

[0084] The results show that using ZrB2 as a substitute for TiB2 in the impregnation composition leads to a significant loss ...

example 3

[0085] The samples used were made of C / C composite material of the same kind as in Example 1, and they were protected against oxidation by modifying the process described in Example 1 as follows:

[0086] in step b), an impregnation composition was used containing, in percentages by weight: 44% of Al (H2PO4)3 and 14% of TiB2 in powder form having a mean grain size of about 10 μm, the remainder being water; and

[0087] in step c), an impregnation composition was used containing, in percentages by weight: 34% of Al (H2PO4)3 and 39% of TiB2 in powder form having a mean grain size equal to about 10 μm.

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Abstract

A part made of a composite material containing carbon, having an open internal residual porosity is protected against oxidation by performing at least one stage in which an impregnating composition is applied, said impregnating composition containing at least one metal phosphate and titanium diboride. Efficient protection against oxidation is thus obtained at temperatures of more than 1000° C., also in the presence of a carbon oxidation catalyst and in a damp medium.

Description

BACKGROUND OF THE INVENTION [0001] The invention relates to providing parts made of composite material containing carbon with protection against oxidation, and in particular parts made of thermostructural composite material comprising carbon fiber reinforcement densified by a matrix that is constituted at least in part by carbon. [0002] Thermostructural composite materials are characterized by their good mechanical properties and by their ability to conserve those properties at high temperatures. Nevertheless, in an oxidizing medium, this ability to conserve good mechanical properties at high temperature depends on the presence of effective protection against oxidation. Whatever the way in which such materials are prepared, they inevitably present residual internal pores that are open and that give oxygen in the surrounding medium access to the core of the material. [0003] In addition, in certain applications, in particular brake disks of carbon / carbon (C / C) composite material as us...

Claims

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Application Information

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IPC IPC(8): C23C22/48C04B41/50C04B41/52C04B41/85C04B41/89F16D69/02
CPCC04B41/009C04B41/5092C04B41/52C04B41/85C04B41/89C04B2111/00362F16D69/023F16D2200/0047C04B41/5031C04B41/5035C04B41/5037C04B41/507C04B35/83F16D69/02
Inventor DISS, PASCALTHEBAULT, JACQUES
Owner MESSIER BUGATTI INC
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